反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
(4-methoxyphenyl)methanamine (0.050 mL, 0.383 mmol) was added to a suspension of a mixture of 8-bromo-6-chloro-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide and a 6,8-dichloro-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide 1E (0.118 g, 0.383 mmol) in tetrahydrofuran (1.0 mL) in a 2 dram screw vial equipped with a stir bar and a teflon coated screw cap. The mixture was heated at 80° C. overnight. The reaction was cooled to room temperature. The reaction was concentrated to dryness under a stream of nitrogen. (trans)-Cyclohexane-1,4-diamine (0.437 g, 3.83 mmol) was added and the mixture was heated to 160° C. After 2 h, the reaction was partitioned between dichloromethane (1.5 mL) and water (1.5 mL). The dichloromethane was removed and concentrated under a stream of nitrogen to provide 6-((trans)-4-aminocyclohexylamino)-8-(4-methoxybenzylamino)-N-(pyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide (0.103 g).
WORKUP
后处理
- temperatureThe reaction was cooled to room temperature
- concentrationThe reaction was concentrated to dryness under a stream of nitrogen
- temperaturethe mixture was heated to 160° C
- customthe reaction was partitioned between dichloromethane (1.5 mL) and water (1.5 mL)
- customThe dichloromethane was removed
- concentrationconcentrated under a stream of nitrogen